THE DEGREE OF CRYSTALLINITY OF MULTICOMPONENT POLYMERS BY X-RAY DIFFRACTION ANALYSIS

Based on the X-ray scattering intensity theory,the correction factors of the degree of crystallinity formulae of the multicomponent polymers have been clearly defined.The formula of degree of erystallinity of the multicomponent polymers was derived in terms of the WAXD theory ahd improved graphic multipeak resolution methods.The results calculated are compatible with the density measurement.

Investigation of Changes in the Fine Structure of Graphitizing Carbon Materials during Heat Treatment by X-Ray Diffraction Analysis

The properties of synthetic graphite materials, widely used in advanced fields, are determined by their structure, which is formed in the process of high-temperature (~2500°C) heat treatment. The fine structure of a graphitizing carbon material based on petroleum coke containing 1.3 wt% S at various stages of graphitization was studied by X-ray diffraction analysis. Some of the samples contained the addition of dispersed Fe2O3. It is shown that the heat-treated material in the range 1200°C - 2600°C is heterogeneous, its component composition is determined by the processing temperature and the presence of Fe2O3 additive. The observed dependence of the component composition on the heat treatment temperature suggests that the process of graphitization of the carbon material, apparently, develops through a number of metastable states.

X-ray diffraction analysis of cold-worked Cu-Ni-Si and Cu-Ni-Si-Cr alloys by Rietveld method

Cold worked and annealed supersaturated Cu-2.65Ni-0.6Si and Cu-2.35Ni-0.6Si-0.6Cr alloys were studied. The microstructural parameters evolution, including crystallite size, root mean square strain and dislocation density was analyzed using Materials Analysis Using Diffraction software （MAUD）. The parameters for both alloys have typical values of cold deformed and subsequently annealed copper based alloy. A net change of the crystallite size, root mean square strain and dislocation density values of the alloys aged at 450 °C for 2.5-3 h seems corresponding to the recovery and recrystallization processes. Addition of Cr as quaternary element did not lead to any drastic changes of post deformation or ageing microstructural parameters and hence of recovery-recrystallization kinetics.

Leaching behavior of phosphorous compounds from sewage sludge ash based on quantitative X-ray diffraction analysis

Phosphorus(P)is an essential and limited resource.Incineration sewage sludge ash(ISSA)contains a high amount of P,which can be recovered using chemical leaching methods.However,the recovery ratio depends on the speciation of P and the leaching conditions.In this study,hydrochloric acid was used as a leaching agent,and the effects of the hydrochloric acid concentration,leaching time,temperature,and liquid-solid ratio on the P leaching ratio were investigated.Furthermore,the co-leaching of macro-metals Ca,Al,Fe,and Mg was analyzed.The results showed that P leached rapidly within 30 min,where the leaching rate reached more than 80%and then gradually stabilized.The leaching concentrations of Ca and Mg had a significant correlation(correlation coefficient r^(2)>0.90),and both were leached completely.Al and P had similar leaching patterns,where the leaching rates increased initially and then decreased with time at 0.2 mol/L HCl.According to X-ray diffraction analysis and Rietveld refinement,the P in ISSA was mainly present in the forms of Mg_(3)Ca_(3)(PO_(4))_(4) and AlPO_(4).When leached using 0.2 mol/L HCl at 55℃ with a liquid-to-solid ratio of 20 L/kg,the AlPO_(4) and Fe_(3)(H_(2)O)_(3)(PO_(4))_(2) in ISSA dissolved initially and then precipitated on the surface of the solid phase,thereby impeding further P leaching.

A New Method for Clay Mineral Analysis and Its Application in Geology

X-ray diffraction (XRD) peaks in a low-angle diffraction section of clayminerals, especially those of authigenic origin, have broadening and tailing features in shape.Using the five basic parameters, peak position, peak height, width, shape coefficient and asymmetry,to describe an XRD peak is more accurate, comprehensive and integrated than using only 3 of them,position, height and width. Following the concept of the five basic parameters of an XRD peak, theprogram Decoform proposed in this study provides more information in mineralogical analyses byfitting actual XRD profiles. In combination with the HW-IR plot, Decoform can he systematically andaccurately used in the comprehensive analyses of crystallinity, domain size, lattice strain andquantitative phase. It is also of value for the geological investigations of diagenesis,metamorphism, basin maturity, structural stress field and so on.

DATA PROCESSING OF UNIVERSAL QUANTITATIVE METHOD IN STANDARDLESS X-RAY PHASE ANALYSIS

Accuracy of coeffcient A_(isp) is related to the reference phase chosen during analysis. The cri- terion of choosing reference phase which may minimize the error of A_(isp) was deduced. The optimum results could be obtained by using the method of least squares if the number of sam- pies for analysis is more than the phase in samples. The procedure presented here is satisfacto- ryfor ordinary phase analysis.

X-ray peak profile analysis of dislocation type,density and crystallite size distribution in cold deformed Pb-Ca-Sn alloys

The density,nature of the dislocations and distribution of the domain sizes in cold-deformed Pb-Ca-Sn solid solution were determined by X-ray diffraction profile analysis.The dislocation densities are of the order of 1010 cm-2.The strain broadening of diffraction profiles was accounted for by dislocation contrast factor.The coherent domain size was determined by the recently developed PM2K software package.Assuming that the domain size distribution is log-normal,the distribution function（median μ and variance σ） was calculated from the size parameters determined from X-ray diffraction profile analysis.

Analysis of the Diffractive Deep Inelastic Scattering Data with Running Coupling and Gluon Number Fluctuations

We study the effects of running coupling and gluon number fluctuations in the latest diffractive deep inelastic scattering data. It is found that the description of the data is improved once the running coupling and gluon number fluctuations are included with x2/d.o.f. = 0.867, x2/d.o.f. = 0.923 and x2/d.o.f. = 0.878 for three different groups of experimental data. The values of diffusive coefficient subtracted from the fit are smaller than the ones obtained by considering only the gluon number fluctuations in our previous studies. The smaller values of the diffusive coefficient are in agreement with the theoretical predictions, where the gluon number fluctuations are suppressed by the running coupling which leads to smaller values of the diffusive coefficient.

Performance of grouts for post-tensioned prestressed structures

New high performance grouts with high volume stability and good fluidity were prepared with Portland cement and a multifunctional admixture (MFA). The theological characteristics and mechanical performance of the grouts were investigated. The addition of MFA effectively improves the pseudo-plasticity of the grout. The Ma cone flow time decreases obviously, and the bleeding rate tends to be zero. The deformation behaviors of fresh mixture and hardened grout are systematically studied. Mercury injection method (MIP), scanning electron microscopy (SEM) and X-ray diffractory analysis experiments are used to analyze the microstructure evolution of the grouts, which manifests that the co-action of the early bubble reaction and the latter ettringite crystallization ensure the volume stability throughout the whole hydration process and result in refined pore structure of the grout.

Microstructure and properties of mullite-based porous ceramics produced from coal fly ash with added Al_2O_3

Using coal fly ash slurry samples supplemented with different amounts of Al2O3, we fabricated mullite-based porous ceramics via a dipping-polymer-replica approach, which is a popular method suitable for industrial application. The microstructure, phase composition, and compressive strength of the sintered samples were investigated. Mullite was identified in all of the prepared materials by X-ray diffraction analysis. The microstructure and compressive strength were strongly influenced by the content of Al2O3. As the Al/Si mole ratio in the starting materials was increased from 0.84 to 2.40, the amount of amorphous phases in the sintered microstructure decreased and the compressive strength of the sintered samples increased. A further increase in the Al2O3content resulted in a decrease in the compressive strength of the sintered samples. The mullite-based porous ceramic with an Al/Si molar ratio of 2.40 exhibited the highest compressive strength and the greatest shrinkage among the investigated samples prepared using coal fly ash as the main starting material. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

Effect of Calcium Leaching on the Properties of Cement-based Composites

Leaching is one of the major factors that alter the mechanical properties of cement-based composites.This study is aimed to investigate the effect of leaching on the properties of cement-based composites.Specimens with two water/cementitious ratios and two mineral admixtures were tested.An electrical potential was applied to accelerate the leaching process.Compressive strength test,scanning electronic microscopy,thermogravimetric analysis and X-ray diffraction analysis were conducted.Test results demonstrated that the calcium leaching reduced compressive strengths of concrete specimens,and such effect was prominent on the specimens without mineral admixtures.The leaching resistance increased with a decrease in water/cementitious ratio and an increase in amount of mineral admixtures.The mineral admixtures would reduce the amount of calcium hydroxide and refine the pore structure through pozzolanic reactions.A fair relationship was found between the calcium leaching and the compressive strength.

Effect of heat treatment on structure and magnetic properties of Fe65.5Cr4Mo4Ga4P12C5B5.5 bulk amorphous alloy

Abstract： This study deals with the Fe65.5Cr4Mo4Ga4P12C5B5.5 ferromagnetic bulk amorphous alloy. XRD analysis showed an amorphous structure of the as-cast sample. The same method revealed that, after annealing at 973 K for v=10 min, the sample displayed a crystalline structure with crystalline phases formed. The crystallization process of the alloy was examined by DTA analysis. It was shown that crystallization took place in the temperature range between 810 K and 860 K with the exo-maximum peak temperature at 846 K with a heating rate of 20 K.min-1. The method also showed that, at temperatures ranging from 753 K to 810 K, the alloy exhibited the properties of supercooled liquids. A correlation between heat-induced structural changes and magnetic properties of the alloy was determined by thermomagnetic measurements. Maximum magnetization M=3.7 Am2.kg-1 of the alloy was reached after its annealing at 733 K for τ=10 min. Upon annealing, the alloy exhibited a relaxed amorphous structure. Annealing the alloy above the crystallization temperature led to a decrease in bulk magnetization. After annealing at 973 K for r=10 min, the bulk magnetization of the alloy was M＇=0.45 Am2.kg-1. Accordingly, after crystallization and formation of new compounds, the magnetization of the alloy was decreased by a factor of about 7.7. The strength of the magnetic field applied during the measurements was H=10 kA.m-1. The samples were tested for changes in the microstructure and hardness of both the amorphous phase and the resulting crystalline phase.

Effects of Yttrium on the Microstructures and Interfaces in a Low Expansion Superalloy

The forms and structures of the phases in Fe-Ni-Co-Nb-Ti-Si low expansion superal-loys have been studied using analytical electron microscopy, high resolution electron microscopy, chemical phase analysis, X-ray diffraction, etc. The effects of yttrium on the microstructures and properties in the superalloys have also been investigated. The results reveal that trace yttrium mainly located in the platelet precipitates makes the crystal structure changed. The platelet precipitates become smaller, denser and rather homogeneous with appropriate yttrium addition. Compared with the conventional low expansion superalloy, the misfit of the platelet phase with the matrix in the yttrium-containing low expansion superalloy decreases from 0.7% to 0.07%, which indicates very low stress at the interface.

Isolation and Crystal Structure of Trans-2,2',4,4'-tetramethyl-6,6'-dinitro Azobenzene

Trans-2,2?,4,4?-tetramethyl-6,6?-dinitro azobenzene (C16H16N4O4, Mr = 328.32) was isolated from benzene extract of the leaves of Aconitum sungpanense Hand. Mazz. as a new compound, and characterized by spectral methods and X-ray diffraction analysis. It crystallizes in monoclinic system, space group P21/c with a = 8.544(1), b = 13.997(2), c = 7.161(1) ? ?= 112.97(1), V = 788.4(2) ?, Z = 4, Dc = 1.383 g/cm3, F(000) = 344 and ?MoKa) = 0.102 mm-1. The final R = 0.0395 and wR = 0.1140 for 1913 independent reflections with Rint = 0.0109 and 1329 observed reflections with I > 2s(I). The molecule is composed of two phenyl rings through trans N=N.

Synthesis of Nickel Sulfide Particles by Solvothermal Process

Pyrite nickel disulfide and millerite nickel monosulfide have been successfully prepared by solvothermal method based on the reaction of Ni(NO3)2.6H2O and H2NC(S)NH2 in benzene and ethylenediamine (EDA). The final products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM). The effects of the solvent, reaction temperature and time on the morphology and phase of the products have been discussed.

Microstructure and optical absorption properties of Au/NiO thin films

Au nanoparticles dispersed NiO composite films were prepared by a chemical solution method.The phase structure,microstructure,surface chemical state,and optical absorption properties of the films were characterized by X-ray diffraction,transmission electron microscopy,X-ray photoelectron spectroscopy,and Uv-vis spectrometer.The results indicate that Au particles with the average diameters of 35-42 nm are approximately spherical and disperse in the NiO matrix.The optical absorption peaks due to the surface plasmon resonance of Au particles shift to the shorter wavelength and intensify with the increase of Au content.The bandwidth narrows when the Au content increases from 8.4wt% to 45.2wt%,but widens by further increasing the Au content from 45.2wt% to 60.5wt%.The band gap Eg increases with the increase of Au contents from 8.4wt% to 45.2wt%,but decreases by further increasing the Au content.

Microstructure and properties of an Al–Ti–Cu–Si brazing alloy for SiC–metal joining

An Al–Ti–Cu–Si solid–liquid dual-phase alloy that exhibits good wettability and appropriate interfacial reaction with SiC at 500–600°C was designed for SiC–metal joining. The microstructure, phases, differential thermal curves, and high-temperature wetting behavior of the alloy were analyzed using scanning electron microscopy, X-ray diffraction analysis, differential scanning calorimetry, and the sessile drop method. The experimental results show that the 76.5Al–8.5Ti–5Cu–10Si alloy is mainly composed of Al–Al2Cu and Al–Si hypoeutectic low-melting-point microstructures (493–586°C) and the high-melting-point intermetallic compound AlTiSi (840°C). The contact angle, determined by high-temperature wetting experiments, is approximately 54°. Furthermore, the wetting interface is smooth and contains no obvious defects. Metallurgical bonding at the interface is attributable to the reaction between Al and Si in the alloy and ceramic, respectively. The formation of the brittle Al4C3phase at the interface is suppressed by the addition of 10wt% Si to the alloy. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

Hydrogenation reaction characteristics and properties of its hydrides for magnetic regenerative material HoCu_2

The hydrogenation reaction characteristics and the properties of its hydrides for the magnetic regenerative material HoCu_2(CeCu_2-type) of a cryocooler were investigated. The XRD testing reveals that the hydrides of HoCu_2 were a mixture of Cu, unknown hydride Ⅰ, and unknown hydride Ⅱ. Based on the PCT(pressure-concentration-temperature) curves under different reaction temperatures, the relationships among reaction temperature, equilibrium pressure, and maximum hydrogen absorption capacity were analyzed and discussed. The enthalpy change ΔH and entropy change ΔS as a result of the whole hydrogenation process were also calculated from the PCT curves. The magnetization and volumetric specific heat capacity of the hydride were also measured by SQUID magnetometer and PPMS, respectively.

Phase diagram of the CsBr-CaBr_2 system

The phase diagram of the CsBr-CaBr2 system was re-determined by using differential thermal analysis and high ternperature and room ternperature X-ray diffraction analysis. It is concluded that there are three intermediate compounds in this system： a.congruently melting compound, CsCaBr3, with a melting point of 823℃ and two incongruently melting compounds, Cs2CaBr4 and Cs3Ca2Br7, whose peritectic points being 597℃ and 635℃, respectively. X-ray diffraction analysis indicated that compound CsCaBr3 is of slightly distorted perovskite structure.

Synthesis and Study of Heteronuclear Citrates

Terms of synthesis were determined for creation of new generation premixes and for their testing in experiments. Heteronuclear chelate citrates of general formula： M12MnL2.nH2O （where, M^I = Zn, Co, Fe, Mn, Cu; MH = Mn, Zn, Co, Cu; n = 0/4） were synthesized. Identity and composition of synthesized compounds were defined by microelemental analysis, determination of melting temperature and X-ray diffraction analysis. X-ray diffraction method was used also to define crystallinity of the compounds and their citric acid （H4L） component. X-ray amorphous and iso-structural orders were also revealed.